反応 #2568

反応方程式

water

N-{2-[4-(4-Fluorobenzoyl)piperidino]ethyl}-4-formyl-N-(2-methoxyphenyl)benzenesulfonamide

hydroxyamine hydrochloride

sodium carbonate

→

title compound

収率 102.7%

N-{2-[4-(4-Fluorobenzoyl)piperidino]ethyl}-4-(N-hydroxyimino)-N-(2-methoxyphenyl)benzenesulfonamide

収率 102.7%

溶媒

ethanol

反応条件

後処理

1. 1
   その他ethanol was removed by evaporation
2. 2
   workup.ADDITIONthe resulting residue was mixed with water (10 ml)
3. 3
   その他to collect crystals
4. 4
   ろ過by filtration
5. 5
   洗浄The thus collected crystals were washed with water and hexane
6. 6
   workup.DISSOLUTIONdissolved in methylene chloride (50 ml)
7. 7
   乾燥dried on anhydrous sodium carbonate
8. 8
   その他Thereafter, the solvent was removed by evaporation

実験手順

N-{2-[4-(4-Fluorobenzoyl)piperidino]ethyl}-4-formyl-N-(2-methoxyphenyl)benzenesulfonamide (63 mg, 0.12 mmol) and hydroxyamine hydrochloride (9.5 mg, 0.132 mmol) were dissolved in ethanol (2 ml) to which were subsequently added anhydrous sodium carbonate (14 mg, 0.132 mmol) and water (1 ml). After 1.5 hours of stirring at room temperature, ethanol was removed by evaporation, and the resulting residue was mixed with water (10 ml) to collect crystals by filtration. The thus collected crystals were washed with water and hexane, dissolved in methylene chloride (50 ml) and then dried on anhydrous sodium carbonate. Thereafter, the solvent was removed by evaporation to obtain 65 mg (100%) of the title compound in the form of colorless powder.

出典